CN108786649A - One kind is by mesoporous SiO2Stable Pickering lotions and preparation method thereof - Google Patents
One kind is by mesoporous SiO2Stable Pickering lotions and preparation method thereof Download PDFInfo
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- CN108786649A CN108786649A CN201810785435.XA CN201810785435A CN108786649A CN 108786649 A CN108786649 A CN 108786649A CN 201810785435 A CN201810785435 A CN 201810785435A CN 108786649 A CN108786649 A CN 108786649A
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Abstract
The present invention relates to one kind by mesoporous SiO2Stable Pickering lotions and preparation method thereof, the Pickering lotions, it includes aqueous surfactant solution, mesoporous SiO2And oil phase substance；Wherein, a concentration of 0.6-3mmol/L of the aqueous surfactant solution；The volume ratio of the aqueous surfactant solution and oil phase substance is 1:1；The mesoporous SiO2Weight is the 0.1%-2% of aqueous surfactant solution weight；The preparation of the Pickering lotions includes the following steps：(1) mesoporous SiO2Preparation；(2) preparation of Pickering lotions；The present invention is by using CTAC as template, having obtained mesoporous SiO2, and obtained the mesoporous SiO being modified with surfactant hydrophobicization2Stable Pickering emulsion systems, stabilization time is more than 100 days to the emulsion system at ambient temperature.
Description
Technical field
The present invention relates to one kind by mesoporous SiO2Stable Pickering lotions and preparation method thereof.
Background technology
Emulsion be a kind of liquid be dispersed in the form of liquid pearl in another liquid immiscible with it and the dispersion that is formed
System.Play an important roll in many industrial process and commercial product.Traditional lotion generally by surfactant or
Person's amphipathic polymer is stablized.However, the cost of usually surfactant is higher, and it is difficult to recycling.
Pickering lotions are to make a kind of New Emulsion of emulsifier with solia particle substitution surfactant, more traditional
Surfactant stablize lotion, have better thermodynamic stability, and low toxicity, it is environmentally friendly.Wherein it is used as emulsification
The solid powder of agent mainly has clay, silica, metal hydroxides, graphite, carbon black etc..In Pickering lotions, when
When particle hydrophily or very strong lipophile, stable lotion cannot be formed.And the commercially available general hydrophily of nano particle is stronger,
So needing that its surface is modified or is modified, the emulsion system to relatively be stablized.Mesoporous material is typically with surface
Activating agent is template, hydrolyzes the intermolecular interaction between presoma by template molecule and organic/inorganic, collaboration is certainly
Assembling forms organic/inorganic composite, is obtained by " sol-gel " method or other methods.Mesoporous material, which is one kind, to be had
High-specific surface area, morphology and size be controllable, duct queueing discipline and the adjustable novel nano-material of pore size, in catalysis, passes
The fields such as sense, absorption have important application.And so far, there is not yet the Pickering breasts stablized with mesoporous nano-grain
Liquid.
Invention content
The purpose of the present invention is to provide a kind of length of stabilization time and by mesoporous SiO2Stable Pickering lotions and its
Preparation method.Using surfactant to mesoporous SiO2Particle surface carries out hydrophobic modification in situ, to form first stability
Pickering lotions.
The purpose of the present invention is achieved through the following technical solutions：One kind is by mesoporous SiO2Stable Pickering lotions, it
Including aqueous surfactant solution, mesoporous SiO2And oil phase substance；Wherein, the aqueous surfactant solution is a concentration of
0.6-3mmol/L；The volume ratio of the aqueous surfactant solution and oil phase substance is 1:1；The mesoporous SiO2Weight be
The 0.1%-2% of aqueous surfactant solution weight.
It is described by mesoporous SiO2The preparation method of stable Pickering lotions, it is comprised the following steps that：
(1) mesoporous SiO2Preparation：With hexadecyltrimethylammonium chloride (CTAC) for template, with tetraethyl orthosilicate
For silicon source the mesoporous SiO is prepared under alkaline medium2；
(2) preparation of Pickering lotions：Surfactant is soluble in water, aqueous surfactant solution is formed, later
Mesoporous SiO is added into aqueous surfactant solution2, ultrasonic disperse, add oil phase substance mix homogeneous to get described
Pickering lotions；
Wherein, a concentration of 0.6-3mmol/L of the aqueous surfactant solution；The aqueous surfactant solution and oil
The volume ratio of phase substance is 1:1；The mesoporous SiO2Weight be aqueous surfactant solution weight 0.1%-2%.
For the prior art, the advantage of the invention is that：The present invention is by using CTAC as template, having obtained one kind
Mesoporous SiO of the grain size in 50-60nm or so2, and obtained the mesoporous SiO being modified with surfactant hydrophobicization2Stable
Pickering emulsion systems.No matter mesoporous SiO2Proportion is how many in system, and the emulsion system is steady at ambient temperature
Fix time can be more than 100 days.The Pickering lotions can expand mesoporous SiO2Application range, while possessing mesoporous spy
Property Pickering lotions can be applied to absorption, separation and catalysis etc. fields.
Description of the drawings
Fig. 1 is the mesoporous SiO of CTAB/2Photomacrograph after stable n-decane/aqueous emulsion system placement 100 days.
Fig. 2 is the mesoporous SiO of CTAB/2Microphoto after stable n-decane/aqueous emulsion system placement 100 days.
Fig. 3 is the mesoporous SiO of Gemini surface active agent 12-2-12/2Stable n-decane/aqueous emulsion system is placed 100 days
Photomacrograph afterwards.
Fig. 4 is the mesoporous SiO of Gemini surface active agent 12-2-12/2Stable n-decane/aqueous emulsion system is placed 100 days
Microphoto afterwards.
Fig. 5 is mesoporous SiO2SEM figure.
Fig. 6 is the mesoporous SiO of 1 gained of embodiment2N2Adsorption-desorption curve, filled symbols represent adsorption curve, hollow
Symbology desorption curve.
Specific implementation mode
The content of present invention is described in detail with embodiment with reference to the accompanying drawings of the specification：
One kind is by mesoporous SiO2Stable Pickering lotions, it includes aqueous surfactant solution, mesoporous SiO2And
Oil phase substance；Wherein, a concentration of 0.6-3mmol/L of the aqueous surfactant solution；The aqueous surfactant solution with
The volume ratio of oil phase substance is 1:1；The mesoporous SiO2Weight be aqueous surfactant solution weight 0.1%-2%.
Surfactant is precisely weighed in sample bottle, ultra-pure water is added, after surfactant is completely dissolved, forms table
Face aqueous surfactant solutions, because the volume of surfactant Surfactant aqueous solution influences little, to be formed surface
The volume of aqueous surfactant solutions is calculated as the volume for the ultra-pure water being added.
Pickering lotions of the present invention are one kind by mesoporous SiO2Change by the hydrophobization in situ of surfactant
Property and the Pickering lotions of stabilization.Using surfactant to mesoporous SiO2Particle surface carries out hydrophobic modification in situ, from
And the Pickering lotions of the stabilization formed, be conducive to mesoporous SiO2In the application of new technical field.
Wherein, the surfactant is quaternary surfactant.The quaternary surfactant is dodecyl
Trimethylammonium bromide, cetyl trimethylammonium bromide (CTAB), Gemini surface active agent 12-2-12, Gemini surface active agent
The mixture of one or more of 12-4-12 or Gemini surface active agent 12-6-12.Wherein, the Gemini surface active agent
The structural formula of 12-2-12, Gemini surface active agent 12-4-12 and Gemini surface active agent 12-6-12 is respectively：
The mesoporous SiO2Be using hexadecyltrimethylammonium chloride as template, using tetraethyl orthosilicate as silicon source,
Under alkaline medium, it is prepared.
The mesoporous SiO2Grain size be 50-60nm.
The oil phase substance is one kind or several in n-decane, soybean oil, olive oil, castor oil, coconut oil or tea oil
The mixture of kind.
It is described by mesoporous SiO2Stable Pickering lotions, its stabilization time are more than 100 days.
It is described by mesoporous SiO2The preparation method of stable Pickering lotions, it is comprised the following steps that：
(1) mesoporous SiO2Preparation：Using hexadecyltrimethylammonium chloride as template, using tetraethyl orthosilicate as silicon
Source is prepared into the mesoporous SiO under alkaline medium2；
(2) preparation of Pickering lotions：Surfactant is soluble in water, aqueous surfactant solution is formed, later
Mesoporous SiO is added into aqueous surfactant solution2, ultrasonic disperse, add oil phase substance mix homogeneous to get described
Pickering lotions；
Wherein, a concentration of 0.6-3mmol/L of the aqueous surfactant solution；The aqueous surfactant solution and oil
The volume ratio of phase substance is 1:1；The mesoporous SiO2Weight be aqueous surfactant solution weight 0.1%-2%.
The concrete operation method of step (1) is：
A. it by the hexadecyltrimethylammonium chloride weighed (CTAC), is dissolved in deionized water, heating stirring to solution
Clarification, obtains hexadecyltrimethylammonium chloride aqueous solution；
B. by the tetraethyl orthosilicate weighed (TEOS) and triethylamine (TEA), at 90-95 DEG C, heating mixing 25-
30min obtains just mixed liquor；
C. the first mixed liquor obtained by step b is added in the hexadecyltrimethylammonium chloride aqueous solution obtained by step a,
Obtain whole mixed liquor, wherein tetraethyl orthosilicate, hexadecyltrimethylammonium chloride, triethylamine and deionization in whole mixed liquor
The molar ratio of water is 1:0.170-0.180:7.9-8.1：110-130；Later, whole mixed liquor is stirred to react 3- at room temperature
5h obtains turbid, i.e. crude product；
D. by the crude product obtained by step c through ethyl alcohol and water washing for several times to neutral, be placed in baking oven, in 60-65
Dry 1-2h at DEG C；Semi-finished product after drying are placed in Muffle furnace, and 550- is to slowly warm up to the heating rate of 1-3 DEG C/min
560 DEG C of roasting 5-6h, obtain mesoporous SiO2。
The concrete operation method of step (2) is：
Surfactant is precisely weighed in sample bottle, ultra-pure water is added, after surfactant is completely dissolved, is added accurate
The mesoporous SiO really weighed2, ultrasonic disperse pipettes oil phase substance in the sample bottle later, then, 11000~
Under conditions of 11500r/min, 2~3min of machinery emulsification is carried out to the system in sample bottle with homogenizer, finally, at room temperature
30~45min is stood to get the Pickering lotions.
Finer elaboration is made to present disclosure with reference to embodiment：
Embodiment 1：Mesoporous SiO2Preparation
A. the CTAC (2.35g, 0.007mol) that certain mass is weighed in eggplant type flask, is dissolved in deionized water
In (90.5g, 5.028mol), heating stirring to solution is clarified, and hexadecyltrimethylammonium chloride aqueous solution is obtained；
B. it weighs a certain amount of TEOS (8.5g, 0.040mol) and TEA (61.2g, 0.410mol) adds at 95 DEG C
Hot mixing heats 25min, obtains just mixed liquor；
C. the first mixed liquor obtained by step b is added in the hexadecyltrimethylammonium chloride aqueous solution obtained by step a,
Obtain whole mixed liquor；Wherein, tetraethyl orthosilicate, hexadecyltrimethylammonium chloride, triethylamine and deionization in whole mixed liquor
The molar ratio of water is 1:0.178:8:120；Later, whole mixed liquor is stirred to react 3h at room temperature, obtains turbid, i.e., thick production
Product；
D. the crude product obtained by step c is extremely neutral for several times through ethyl alcohol and water washing, it is placed in baking oven, in 60 DEG C of dryings
1h；Semi-finished product after drying are placed in Muffle furnace, are to slowly warm up to 550 DEG C of roasting 5h with the heating rate of 2 DEG C/min, are situated between
Hole SiO2。
As shown in Figure 5, the mesoporous SiO of gained2The grain size of particle is distributed more uniform in 50nm or so.
Fig. 6 is the mesoporous SiO of 1 gained of embodiment2N2Adsorption/desorption curve, the curve are IV types, i.e. desorption curve and suction
Attached curve is inconsistent, hysteresis loop occurs, is typical mesoporous material adsorption desorption curve, illustrates that embodiment 1 prepares mesoporous
Material has meso-hole structure.
Embodiment 2：Mesoporous SiO2Preparation
A. the CTAC (2.18g, 0.0068mol) that certain mass is weighed in eggplant type flask, is dissolved in deionized water
In (79.2g, 4.4mol), heating stirring to solution is clarified, and hexadecyltrimethylammonium chloride aqueous solution is obtained；
B. it weighs a certain amount of TEOS (8.3g, 0.040mol) and TEA (47.2g, 0.316mol) adds at 90 DEG C
Hot mixing heats 30min, obtains just mixed liquor；
C. the first mixed liquor obtained by step b is added in the hexadecyltrimethylammonium chloride aqueous solution obtained by step a,
Obtain whole mixed liquor；Wherein, tetraethyl orthosilicate, hexadecyltrimethylammonium chloride, triethylamine and deionization in whole mixed liquor
The molar ratio of water is 1:0.170:7.9：110；
Later, whole mixed liquor is stirred to react 5h at room temperature, obtains turbid, i.e. crude product；
D. the crude product obtained by step c is extremely neutral for several times through ethyl alcohol and water washing, it is placed in baking oven, in 65 DEG C of dryings
2h；Semi-finished product after drying are placed in Muffle furnace, are to slowly warm up to 560 DEG C of roasting 6h with the heating rate of 1 DEG C/min, are situated between
Hole SiO2.The mesoporous SiO of gained2The grain size of particle in 60nm or so,
Embodiment 3：Mesoporous SiO2Preparation
A. the CTAC (2.30g, 0.0072mol) that certain mass is weighed in eggplant type flask, is dissolved in deionized water
In (93.6g, 5.2mol), heating stirring to solution is clarified, and hexadecyltrimethylammonium chloride aqueous solution is obtained；
B. it weighs a certain amount of TEOS (8.3g, 0.040mol) and TEA (48.4g, 0.324mol) adds at 92 DEG C
Hot mixing heats 28min, obtains just mixed liquor；
C. the first mixed liquor obtained by step b is added in the hexadecyltrimethylammonium chloride aqueous solution obtained by step a,
Obtain whole mixed liquor；Wherein, tetraethyl orthosilicate, hexadecyltrimethylammonium chloride, triethylamine and deionization in whole mixed liquor
The molar ratio of water is 1:0.180:8.1：130；Later, whole mixed liquor is stirred to react 4h at room temperature, obtains turbid, i.e., thick production
Product；
D. the crude product obtained by step c is extremely neutral for several times through ethyl alcohol and water washing, it is placed in baking oven, in 62 DEG C of dryings
1.5h；Semi-finished product after drying are placed in Muffle furnace, are to slowly warm up to 555 DEG C of roasting 5.5h with the heating rate of 3 DEG C/min, are obtained
To mesoporous SiO2.The mesoporous SiO of gained2The grain size of particle in 55nm or so,
Embodiment 4：The system of the Pickering lotions of hydrophobic modification is carried out with CTAB (cetyl trimethylammonium bromide)
It is standby：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 0.6mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 0.5%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
Embodiment 5：The system of the Pickering lotions of hydrophobic modification is carried out with CTAB (cetyl trimethylammonium bromide)
It is standby：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 0.9mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 0.5%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
Embodiment 6：The system of the Pickering lotions of hydrophobic modification is carried out with CTAB (cetyl trimethylammonium bromide)
It is standby：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 1mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 0.5%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
Embodiment 7：The system of the Pickering lotions of hydrophobic modification is carried out with CTAB (cetyl trimethylammonium bromide)
It is standby：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 2mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 0.5%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
Embodiment 8：The system of the Pickering lotions of hydrophobic modification is carried out with CTAB (cetyl trimethylammonium bromide)
It is standby：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 3mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 0.5%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
If Fig. 1 is the mesoporous SiO of CTAB/ that embodiment 4-8 is recorded2Stable n-decane/aqueous emulsion system is placed 100 days
Photomacrograph afterwards, be followed successively by from left to right in Fig. 1 embodiment 4, embodiment 5, embodiment 6, embodiment 7, made from embodiment 8
Pickering lotions, and the concentration of CTAB aqueous solutions used from left to right be followed successively by 0.6mmol/L, 0.9mmol/L,
1mmol/L,2mmol/L,3mmol/L.From fig. 1, it can be seen that after these Pickering lotions are placed 100 days, still keep fabulous
Stability is macroscopically precipitated without oil phase.
Fig. 2 is the mesoporous SiO of CTAB/ of embodiment 4-8 records2After stable n-decane/aqueous emulsion system is placed 100 days
Microphoto.Wherein, figure a, b, c, d, e in Fig. 2 are respectively embodiment 4, embodiment 5, embodiment 6, embodiment 7, implement
The microphoto of Pickering lotions made from example 8, and scheme the CTAB concentration of aqueous solution difference used in a, b, c, d, e
0.6mmol/L,0.9mmol/L,1mmol/L,2mmol/L,3mmol/L；
From figure 2 it can be seen that when CTAB concentration of aqueous solution is 0.6mmol/L, the drop of the Pickering lotions of formation
Grain size is 29 μm, and size droplet diameter distribution is more uniform；
When CTAB concentration of aqueous solution is 0.9mmol/L, the size droplet diameter of the Pickering lotions of formation is 33.5 μm, and
Size droplet diameter distribution is more uniform；
When CTAB concentration of aqueous solution is 1mmol/L, the size droplet diameter of the Pickering lotions of formation is 19.5 μm, and liquid
It is more uniform to drip particle diameter distribution；
When CTAB concentration of aqueous solution is 2mmol/L, the size droplet diameter of the Pickering lotions of formation is 11.8 μm, and liquid
It is more uniform to drip particle diameter distribution；
When CTAB concentration of aqueous solution is 3mmol/L, the size droplet diameter of the Pickering lotions of formation is 18 μm, and drop
Particle diameter distribution is more uniform；
Embodiment 9：The system of the Pickering lotions of hydrophobic modification is carried out with CTAB (cetyl trimethylammonium bromide)
It is standby：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 2mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 0.1%；
The soybean oil for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11500r/min, uses
Homogenizer carries out machinery emulsification 3min to system, finally, stands 45min at room temperature to get the Pickering lotions.
Embodiment 10：The Pickering lotions of hydrophobic modification are carried out with CTAB (cetyl trimethylammonium bromide)
It prepares：
CTAB is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, after CTAB is completely dissolved, is formed dense
Degree is the CTAB aqueous solutions of 3mmol/L；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be CTAB aqueous solution weight 2%；
The castor oil for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11200r/min, uses
Homogenizer carries out machinery emulsification 3min to system, finally, stands 40min at room temperature to get the Pickering lotions.
Embodiment 11：With the preparation of the Gemini surface active agent 12-2-12 Pickering lotions stablized.
Gemini surface active agent 12-2-12 is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, waits for Shuangzi
After surfactant 12-2-12 is completely dissolved, the Gemini surface active agent 12-2-12 aqueous solutions of a concentration of 1.5mmol/L are formed；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be Gemini surface active agent 12-2-12 aqueous solution weight 0.6%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
Embodiment 12：With the preparation of the Gemini surface active agent 12-2-12 Pickering lotions stablized.
Gemini surface active agent 12-2-12 is precisely weighed in the sample bottle of 10mL, the ultra-pure water of 4mL is added, waits for Shuangzi
After surfactant 12-2-12 is completely dissolved, the Gemini surface active agent 12-2-12 aqueous solutions of a concentration of 3mmol/L are formed；
Then the mesoporous SiO of 1 gained of embodiment is accurately weighed again2In the sample bottle, ultrasonic disperse；Its intermediary hole
SiO2Weight be Gemini surface active agent 12-2-12 aqueous solution weight 0.6%；
The n-decane for pipetting 4mL later is used as oil phase substance in the sample bottle, under conditions of 11000r/min, uses
Homogenizer carries out machinery emulsification 2min to system, finally, stands 30min at room temperature to get the Pickering lotions.It is right
The macrostate of Pickering lotions carries out shooting record, and super depth-of-field microscope is used in combination to shoot its displaing micro picture.
Such as the mesoporous SiO of Gemini surface active agent 12-2-12/ that Fig. 3 is embodiment 11, embodiment 12 records2It is stable just
Decane/aqueous emulsion system place 100 days after photomacrograph, be followed successively by embodiment 11 from left to right in Fig. 3, embodiment 12 is made
The Pickering lotions obtained, and the concentration of Gemini surface active agent 12-2-12 aqueous solutions used from left to right is followed successively by
1.5mmol/L,3mmol/L.As can be seen from Figure 3, after these Pickering lotions are placed 100 days, fabulous stabilization is still kept
Property, macroscopically it is precipitated without oil phase.
The mesoporous SiO of Gemini surface active agent 12-2-12/ that Fig. 4 is embodiment 11, embodiment 12 records2The stable positive last of the ten Heavenly stems
Microphoto after alkane/aqueous emulsion system placement 100 days.Wherein, figure a, b in Fig. 4 are respectively embodiment 11, embodiment 12
The microphoto of Pickering lotions obtained, and scheme the Gemini surface active agent 12-2-12 concentration of aqueous solution point used in a, b
Other 1.5mmol/L, 3mmol/L；
Figure 4, it is seen that when Gemini surface active agent 12-2-12 concentration of aqueous solution is 1.5mmol/L, formation
The size droplet diameter of Pickering lotions is 27.5 μm, and size droplet diameter distribution is more uniform；
When Gemini surface active agent 12-2-12 concentration of aqueous solution is 3mmol/L, the drop of the Pickering lotions of formation
Grain size is 10 μm, and size droplet diameter distribution is more uniform；
The bound value and interval value of each raw material of the present invention can realize the present invention and cited each raw material all
It can realize the present invention, embodiment is just not listed one by one herein.
It should be noted that heretofore described is specific embodiments of the present invention and technical principle, this hair is being read
After bright the above, those skilled in the art can be used for various modifications and be modified without departing from the present invention's to the present invention
Range, such equivalent forms are also fallen in the scope of the present invention.
Claims (10)
1. one kind is by mesoporous SiO2Stable Pickering lotions, it is characterised in that：It includes aqueous surfactant solution, mesoporous
SiO2And oil phase substance；Wherein, a concentration of 0.6-3mmol/L of the aqueous surfactant solution；The surfactant
The volume ratio of aqueous solution and oil phase substance is 1:1；The mesoporous SiO2Weight be aqueous surfactant solution weight
0.1%-2%.
2. according to claim 1 by mesoporous SiO2Stable Pickering lotions, it is characterised in that：The surface-active
Agent is quaternary surfactant.
3. according to claim 2 by mesoporous SiO2Stable Pickering lotions, it is characterised in that：The quaternary ammonium salt table
Face activating agent is dodecyl trimethyl ammonium bromide, cetyl trimethylammonium bromide, Gemini surface active agent 12-2-12, double
The mixture of one or more of sub- surfactant 12-4-12 or Gemini surface active agent 12-6-12；Wherein, described double
The structural formula of sub- surfactant 12-2-12, Gemini surface active agent 12-4-12 and Gemini surface active agent 12-6-12 point
It is not：
4. according to claim 1 by mesoporous SiO2Stable Pickering lotions, it is characterised in that：The mesoporous SiO2
It is, using tetraethyl orthosilicate as silicon source, under alkaline medium, to be prepared using hexadecyltrimethylammonium chloride as template
's.
5. according to claim 1 by mesoporous SiO2Stable Pickering lotions, it is characterised in that：The mesoporous SiO2
Grain size be 50-60nm.
6. according to claim 1 by mesoporous SiO2Stable Pickering lotions, it is characterised in that：The oil phase substance
For the mixture of one or more of n-decane, soybean oil, olive oil, castor oil, coconut oil or tea oil.
7. according to claim 1 by mesoporous SiO2Stable Pickering lotions, it is characterised in that：Its stabilization time
More than 100 days.
8. according to claim 1-7 any one by mesoporous SiO2The preparation method of stable Pickering lotions,
It is characterized in that：It is comprised the following steps that：
(1) mesoporous SiO2Preparation：Using hexadecyltrimethylammonium chloride as template, using tetraethyl orthosilicate as silicon source, in alkali
Under property medium, it is prepared into the mesoporous SiO2；
(2) preparation of Pickering lotions：Surfactant is soluble in water, formed aqueous surfactant solution, backward table
Mesoporous SiO is added in the aqueous surfactant solutions of face2, ultrasonic disperse, add oil phase substance mix homogeneous to get described
Pickering lotions；
Wherein, a concentration of 0.6-3mmol/L of the aqueous surfactant solution；The aqueous surfactant solution and oil phase thing
The volume ratio of matter is 1:1；The mesoporous SiO2Weight be aqueous surfactant solution weight 0.1%-2%.
9. according to claim 8 by mesoporous SiO2The preparation method of stable Pickering lotions, it is characterised in that：Step
Suddenly the concrete operation method of (1) is：
A. the hexadecyltrimethylammonium chloride that will be weighed, is dissolved in deionized water, and heating stirring to solution is clarified, and obtains 16
Alkyl trimethyl ammonium chloride aqueous solution；
B. by the tetraethyl orthosilicate weighed and triethylamine, at 90-95 DEG C, heating mixing 25-30min obtains just mixed liquor；
C. the first mixed liquor obtained by step b is added in the hexadecyltrimethylammonium chloride aqueous solution obtained by step a, obtains end
Mixed liquor, wherein tetraethyl orthosilicate in whole mixed liquor, hexadecyltrimethylammonium chloride, triethylamine and deionized water
Molar ratio is 1:0.170-0.180:7.9-8.1：110-130；Later, whole mixed liquor is stirred to react 3-5h at room temperature, obtained
To turbid, i.e. crude product；
D. by the crude product obtained by step c through ethyl alcohol and water washing for several times to neutral, be placed in baking oven, at 60-65 DEG C
Dry 1-2h；Semi-finished product after drying are placed in Muffle furnace, and 550-560 DEG C is to slowly warm up to the heating rate of 1-3 DEG C/min
5-6h is roasted, mesoporous SiO is obtained2。
10. according to claim 8 by mesoporous SiO2The preparation method of stable Pickering lotions, it is characterised in that：
The concrete operation method of step (2) is：
Surfactant is precisely weighed in sample bottle, ultra-pure water is added, after surfactant is completely dissolved, accurate claim is added
The mesoporous SiO taken2, ultrasonic disperse pipettes oil phase substance in the sample bottle, then, in 11000~11500r/min later
Under conditions of, 2~3min of machinery emulsification is carried out to the system in sample bottle with homogenizer, finally, at room temperature stand 30~
45min is to get the Pickering lotions.
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